Sylvania



May 1"5, 1923.

F. F. MARQUARD ET Al.

METHOD OF EVAPORATING AMMONIA LIQUOR Filed Nov. ll, 1920` 2 Sheets-Sheet l May 15, 1923. K 1,455,299

F. F. MARQUARD ET AL METHOD OF EVAPORATING AMMONIA LIQUOR Filed Nov, 11, 1920 2 sheets-sheet 2 a #ar/7 ry Patented May 15, i923.

tisana.

uNrrsn sra'ras PATENT i orties,

FRANK. r. Man-enano, or cnarn'roN, vAND cani. W. merrain, or swrssvntn, PENN- sYLvANn-i. f i

Application filed November 11, 1920. Serial No. 423,228.

To au whom t may concern Be it known that we, FRANK F. Maa Quinn) and Gann WV. Lrrrnnn, both citizens of the United States, and residents, yrespectively, of Clairton and Swissvale, both in the county of Allegheny vand State of Pennsylvania,have inventedcertain new and usei ful Improvements in Methods of EvaporatingAmmonia Liquor, of which the following is a specification. l

This invention relates to the recovery of ammonium chloride, and other similar sol-l uble salts, froinweak ammonia liquor, ask

derived from the operation of by-product coke plants, and relates particularly to a novel method for treatin@ ythe li uor to re-l be circulated from the basin into the top ofy the tower and allowedy to fall against a forced counter-flow of the products of com'- bustion. The liquor during its continued and repeated circulation through. the tower will give up all waterw and soluble tar vapors to the forced draft of products of combus tion and become either evaporated .entirely or circulated until it reaches the point of saturation when the salts willbe precipitated in the solution which is held in the basin at the lower end of the tower.

The above apparatus and method will produce an economy in heat requirements, purification of liquor by aeration, and many other advantages that will be more fully set forth in the following description.

inthe accompanying drawings, Figurel l' is a somewhat diagrammatic sectional side elevation of a complete apparatus.

Figure la is to be joined to Figure 1 on the line X-X to form a complete sectional elevation.

Figure 2 view of the tower showing one of the banks of baiiies in position.

ris an enlarged cross-sectional Figure 3 is an enlarged fragmentary side elevation showing several banks of battles.

` Referring particularly to the drawings, the letter ii designates the furnace as a whole, and the letter l?) designates the tower. rlfhe n furnace and tower are preferably formed from brick and are built integral, the tower serving as a flue or stack for the furnace. l 1

y The furnace ii. is of ordinary construction and is composed of top and bottom walls 2 and 3, front wall 1l, 'and side walls o. A checker-wall Y is arranged within the furnace adjacent its rear end, and a lirewall 8 is arranged immediately forward of the checkenwall 7. flic fire-wall 8 is of considerable depth and spaced from thev top wall 2 forming a passage 8*l for the .products of combustion and forced draft, which pass onward through the checker-wall 7 and into the tower B. i

A conc yete base`9 is provided for the furnace A and tower B. The furnace portion of the l ase extends a considerable distance beyond the furnace ,inland is formed hollow rso as 'to provide an air duct l0, which has its forward end in communication with a llower 13 driven by a suitable motor it. kuitable air conduits ll are formed in the lire-wall and have their lower ends opening into the air. duct l() to supply a forced draft. v l

A ny suitable fuel may be used to lire the furnace A, although gas is the preterred fuel, and therefore, a burner l2 has been shown communicating through' the front wall l with the interior of the furnace, and having air supply tubes 12a extending downward and communicating with air duct i0.

A damper ,A isprovided in the air duct l() to regulate'the flow of air to the air conduits ll, and a seeondaryair duct 15 is provided to aomit air to the rear of the duct vl0 vif desired or necessary.

The tower B comprises front and back walls 16 and 1'." and'side walls i8 and 19, kand a bottom wall 20, and extends a consideraale distance below the furnace il to provide a basin forfthe reception of the liquor being evaporated, The basin or lowerportion of the tower is divided into two parts or chambers K and Y by a transverse wall 2l for the reception of liquids of diiferent qualities.

The back wall 17 has a cutaway portion at its bottom forming an outlet opening into a` settling chamber or basin 23, which is provided with a depression in its bottom so as to allow for complete drainage ot all liquid. f

Spaced at intervals along the length ot the tower from a point considerably above the top oit the furnace, are a plurality ot baille supports 25, which are composed o' wood or other non-corrosive material. The supports are spaced so as to term upper and lower units or groups, and each support is mounted rigidly in the side walls ot the tower to support suitable battles C.

rlhe bellies C are composed ci bottom and top layers of sections 26, each section being composed or a plurality ot slats 26 set edgewise and spaced by separators or spacers 25,` and held together by sui yable pins 27 which pass through the slats and separators and have wedges 28 passing through their ends to bind the parts together. The under sides of the slats 26 are notched at 29 to fit over the supports 25, and further cut away to form a plurality ot drip points 36.

The sections 26 `forming the lower layer are supported directly upon the supports 25, and the slats extend at right angles to said supports, while the sections 26C of the top layer are supported on the lower sections and extend the opposite direction or at right angles to the sections of the bottom layer, thereby forming a checker-like baille.

'The bailies C are composed completely ot wood or other noircorrosive material.

rlhe liquor which is treated in the upper portion ot the tower and which will lall or be sprayed over the upper unit or group oic bailles is of dierent quality than that to be treated in the lower portion, and therefore, is caught before it falls onto the lower unit or group of baffles in an annular trough 32. Av suitable cone-shaped shield 33 is arranged centrally within the tower and spaced above the trough 32, and has its lower edges overlying the inner edge of the trough so as to direct the liquor into the trough.

Adeflecting shield or baille plate 35 is se-` cured to the front wall 16 ot the tower,

y slightly above the furnace A., and extends downwardly and inwardly on an angle, so as to deiect a spray ot liquor in sheet torination past the mouth ot the 'furnace A and into the chamber X ot the tower, thereby preventing he volatilization of the aminonium chloride, and further providing a means of regulating the temperature of the gases entering the stack by spraying difterent quantities ot liquor onto the detlecting shield or baule plate. l

A second shield or battle plate 36 is secured above the shield 35 and extends inwardly and downwardly ons greater angle than the shield 35 so as to overlie the same and rethe tower.

The liquor to be treated, which is termed veal; liquor, enters the chamber X ot the tower A through a suitable inlet 3T and is drawn from the chamber X by a pump 33 having an inlet pipe 39 communicating with the chamber. rlhe pump 38 'forces the weak liquor upwardly through a main 40 ruiming parallel with the rear wall ot the tower. A suitable branch pipe 4l is connected with the pipe 40 and is provided with a nozzle 42 to provide a spray ot weak liquor against the shield 35.

A suitable pump 44 having inlet pipes and 46 communicating with the chamber Y and settling basin 23 respectively, is provided to draw the saturated or already treated liquor from the chamber Y and settling basin 23, and to torce said liquor upwardly through a main 47 which extends the entire height and parallel with the tower.

A suitable valved branch connection 43 leads from both of the mains 40 and 47 to a suitable manifold distributor 49, having a plurality ot sprays 50 adapted to spray liquor over the lower unit ot bailles.

The main 40 is connected with the main 47 at a point above the branch 48, and the main 47 is provided with a valve 5l below this connection so that the flow of liquor from pump 44 will normally be shut trom this portion ot the main.

A second manifold distributor 52 having a plurality of sprays 53 is provided to spray liquor from the top of the tower over the upper unit or baffles. The manifold distributor is connected with the upper end ot main 47 by a branch 55.

At a point below the lowermost hurdle C, or in the hot zone, a plurality ot spray nozzles 56 extend through the walls of the tower. Nozzles 56 are connected to a supply pipe 57 which is connected to the mains 40 and 47 by suitable valved connections 58, and are adapted to normally take their supply from the main 47, thereby spraying saturated liquor into the products ot combustion and against the lower baliies, to protect said barriles against disintegration due to overheating, and such spray also serving to turther condense the liquor.

The spraying of .weak liquor through the sprays serves to condense the liquor, and also to wash down any traces of ammonium chloride in the term ot salt carried up inechanically by outgoing vapors and the products oitl combustion. The condensed liquor and salts itrom the upper unit of balies Stalls into the trough 32 and is conveyed a main 6() downward into the settling basin 23.

n. suitable salt ejector and salt boxA 65 is arranged above the settling chamber 23 to remove the salt therefrom'. Any suitable through a branch A plurality of manholes 6G are provided inthe back wall 1? et 'the tower to' provide ready laccess to theinterior of thetower, toi' remoijal ot lthe collected and formed salts or to malte repairs or adyustments;

According to oui'ymethod ak quantity 'of raw orwe'alr liquor is yadmitted to the chaniber X of the tower B, through the inlet 37.'

'llie pump 3S is then set in operation to draw the liquor from this chamber and torce it upwardly through the mainv40.

rl"hc valv'ed connections 48 and 58 are justed so that liquor i'roin the main 40 will lowtherethrough and into the spraysoO and nozzles 56, respectively. Thenozzle 42 is connected atv all timeswithy the' mainv 40 4l, thereby providing a spray o' raw or wealr yliquor against the shield 35. The valve v51 inthe main 47`is normally closed and the main is in open communication ywith the niain 47. here- 'fore the upper portion of main 47 will convey a weak liquor tothe manifloldr chamber y y oorrodible vbailles, and passing a counter- 52 and sprays 53. y l

vThe furnace A is fired when thepumpf .is started, thereby ,producing a quantity 'of liet gases which will pass `through into the tower B and rise to meet the down coming liouor. Air is forced through 'the air duct lOand inlets 1lv while the furnace `is in operf ation, therebycreatinig a draft to force the products ol combustion and hot ,gases up through the towerB.

The liquor being sprayed into' the tower through ythe saravs and nozzles '56 will 7 y tall onto the shield 36 and be directed into the chamber Y, whilel the liquor sprayed through the sprays 53 will 'fall over the upper unit oit/battles and into the trough 32 from which it will be conducted into the settling basin 23.

As the liquor is sprayed into the tower it must :tall against the counter-current of hot gases, which cause it to gire up its water and soluble tar vapors, Jr'orming a concentrated solution andsalt crystals. f

Als the chamber Y becomes sufficiently filled with concentrated and salt ladened liquor, the pump 44 is started in motion to torce the concentrated and salt ladened liquor into the main 4'?, and "the valved connections 48 and 58 are adjusted so that the nozzles 56 will receive their supply entirely 'from the main 47, and the sprays 50 will receive a mixed supply from both mains-40 and 47.

The apparatus will then re-circulate the` rlheretore, anordinary forni of ap' against said counterlow or hot X by means of the pump 38 which will torce it through the mains 40 and upper portiono vmain 47, such .liquorbeing mixed with the saturatedliquor troininaln 47, in the sprays 5l), 'and being fed exclusively through the sprays The liquor lroin the sprays 53 is vcoi'icentrated as it falls over the ballles C in thegupper unit, and also is saturatedwith salt crystals carried upwardly mechanically' by the hot gases and is, therefore, conducted directly into the settling chamber 2B.

yAs the liquors become saturated, the salts are removed in any desired manner from the settling basin 28. Preferably the ejector will be employed to'orce the salts from the basin 23 into the salt boi: 65. f-

' The above method vrequires less heat, causes a Amore ellicient puriication of the liquors by aeration, and concentrates the liquors to thedesired degree in less time than any method` employed or known heretofore.

lWe claim l. The method of treating crude ammonia liquor. from by-product colte plants to reycover the salts of ammonium chloride and other salts therein, which consists in passing such liquordown through a tower over nonlow of hot iras up through saidtower, spraying a quantity vof the liquor into the path of said hotgas and up against the lower bai'n fles, collecting all 'or' said liquor in the lowery portion ofthe tower, and passing said liquor in a Icontinuous'circuit from thebottom of the tower upward through suitable conduits and spraying it down over. said' ba'illes gas, causing .it to evaporate until the desired degree of concentration is'elfected.

2. rEhe method of treating` crude ammonia liquor from by-product coke plants to recover the ysalts of ammonium chloride and `other salts therein, which consists in proit into the tower' so as to cause it to pass down through said tower over a plurality of non-corrodible ballles, passing a counteriiow of hotgases up through said tower to concentrate said liquor to the desired degree, and spraying a quantity of the liquor into the path of said hot gases and up vagainst the lower baffles to protect them from linqury by the hot gases and to prevent salting thereon. l

rllhe method. of treating crude ammonia liquor, from by-product coke plants to recover the saltsv of ammonium chloride and other salts therein, which consists in provid -ing a body of said liquor in ay basin at the lower end of a tower, continuously circulan ing said liquor upwardly through suitable conduits along said tower and spraying it corrodible baitles, passing a counter-flow of hot gases up through said tower, causing partial evaporation, and aeration of saidV liquors, thereby concentrating it to the desired degree, and spraying a quantity of the liquor o the path ot' said h ot gases and up against the lower battles to protect them trom in iury by the hot gases and to prevent salting` thereon.

l-. rlhe method of treating crude ammonia liquor trom `by-product coke plants to recover the salts ot ammonium chloride and other salts therein, which consists in passing a weak `iolution or' said liquor into a cham ber of the basin of an evaporating tower, passing said liquid upward to the top of said tower and spraying` it down over a series ot non-corrodible battles in said tower against a counter-flow oit hot gases toy concentrate it, collecting said concentrated liquor and conducting to a settling chamber, and continuously re-circulating said concentrated liquor by conducting it upwardly along a. portion of said tower, and spraying it` over lower series of non-corrodible battles in said tower against a counter-How or' hot gases to further concentrate it until the desired degree of saturation is obtained.

The method oit treating crude ammonia liquor from by-product coke plants to recover the salts oi ammonium chloride and other salts therein, which Aconsists in passing av weak solution or said liquor into a chamber of the basin of an evaporating tower, continuously circulating a concentrated solution ot said liquor from a second chamber in said basin upwardly along a portion of said tower and spraying it'over a lower Series et non-.corrodiblc baffles in said tower, providing a forced counter-flow of hot gases from a furnace communicating with said tower adjacent its lower end, conducting said waal; liquor from said C "s i: ist named chamber upward to the top of said tower and spraying it down over an upper series of non-corrodible battles in said tower against said counter-flow of gases, said weak liquor being concentrated by the action of said gases and also serving t wash down any traces ot salts carried up mechanically by iup-going; gases and vapors, trapping said w alr liquor 'at a point above said lower series of baiiles, and conducting it to Said basin,

6. lhe method of treating crude ammonia liquor from by-product coke plants to recover the salts of ammonium chloride and other salts therein, which consists in passing a weak solutionof said liquor into a chamber oi the basin of an evaporating tower, continuously circulating` a concentrated solution of said liquor from a second chamber in said basin upwardly along a portion of said tower and spraying it over a lower series of non-corrodible battles in said tower, providing a forced countertlow of hot gases from a furnace communicating with said tower vadj acent its lower end, conducting said weak liquor from said first named chamber upward to the top Of said tower and spraying it down over an upper series of noncorrodible baiiies in said tower against said counter-flow, of hot `gases, said weak liquor being concentrated by the action of said gases and also serving to wash down any traces of salts carried up mechanically by upgoing gases and vapors, trapping said liquor after it has passed over said upper series of batlies at a point above said lower series of baliles and conducting it to said basin, and spraying a quantity of liquor in a. flat sheet formation across the entrance of said counter-flow ot hot gases to regulate the flow of said gases. v

' In witness whereof, we have hereunto signed our names.

FRANK F. MARQUARD. CARL XV. LITTLER. 

